IS 13981 : 1994 ( Reaffirmed 2003 ) Indian Standard BENZOTHIAZYL-N-MORPHOLINYL SULPHENAMIDE ( MBS > - SPECIFICATIQN UDC 678'4'044'472 @ BIS 1994 BUREAU MANAK April 1994 OF BHAVAN, INDIAN STANDARDS ZAFAR MARG Price Group 2 9 BAHADUR SHAH NEW DELHI 110002 Rubber Products Sectional Committee, PCD 13 FOREWORD This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Rubber Products Sectional Committee, hzd been approved by the Petroleum, Coal and Related Products Division Council. Benzothiazyl-N-morpholinyl sulphenamide ( MBS > is a well known onset of cure for various applications in the rubber industry. accelerator with a delayed It is soluble in benzene, toluene, carbon tetrachloride, acetone, ethyl ether, chloroform, ethanol In order to facilitate proper application of this member of the sulphenaand insoluble in water. mide class of accelerators in the rubber industry, this standard indicating chemical requirement and technological evaluation procedure has been brought out. Like all other sulphenamide, this sulphenamide accelerator is sensitive to degradation and loss of With time, this material degrades releasing amine showing a loss activity on long storage periods. in assay content and an increase in methanol insoluble due to the formation of MBIS. Use of degraded sulphenamide in rubber compounds will cause decrease in the scorch safety, cure rate Heat, humidity and acidic conditions increase the rate of degradation of and state of cure. sulphenamides and hence this type of material should be stored in a cool and dry place and away from any acidic material or atmosphere. The material being a reactive chemical, all persons concerned with handling of this chemical should be thoroughly informed about the nature of the material, possible effect on contact, inhalation and accidental ingestion. For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance wlth IS 2 : 1960 `Rules for rounding off numerical values (revised)`. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard. iS 13981 :%994' $ Indian St&dard ; ' BENZOTHIAZYL-N-MO RPHOLINYL SULPHENAMIDE ( MBS ) - SPECIFICATION 1 SCOPE IS No. 7086 Title This standard prescribes the requirements and methods of sampling and test for benzothiazylN-morpholinyl sulphenamide ( MBS > intended for use in rubber compounding as a delayed action accelerator. The standard is applicable for msterial in powder or granular or pellet form. 2 NORMATIVE REFERENCES ( Part 1 > : 1973 8851 : 1994 3 REQUIREMENTS 3.1 Description Methods of sampling and test for rubber compounding ingredients, Part 1 Sulphur for rubber industry (first revision ) The following standards contain provisions which through reference in this text, constitute provisions of the standard. At the time of publication, the editions indicated were va.lid. All standards are subject to revision, and parties to agreements based on the standard are encouraged to investigate the possibility of applying the most recent edition of the standards indicated below: The material shall be in the form of light creamy grey powder or granule or pellet form having relative density of about 1.3 ( for guidance only > and shall be free from visible impurities. Th.e material in the form of granules/pellets may be treated with dusting or binding agents. 3.2 The material shall also comply with the requirements given in Table 1 when tested according to the procedures given in co1 4 of Table 1. Table 1 Requirements of Benzothiazyl-NMorpbolinyl Sulphenamide ( MBS ) G. Characteristics Requirement (3) 82 0.5 20 o-75 Metbod of Test, Ref to (4) A-3 of IS 6918 : 1972 A-6 of IS 6918 : 1972 A-7 of IS 6918 : 1972 Annex A IS No. 6070 : 1992 1675 ~: 1971 3399 : 1994 3400 ( Part 1 ) : 1987 Reagent revision > Title grade water ( third (first . Stearic acid, technical revision > Zinc oxide for rubber industry ( second revision ) Methods of test for vulcanized rubbers : Part 1 Tensile properties strain stress ( second revision ) Methods canized Hardness of test for vulrubbers : Part 2 revision > (1) (2) i) Melting point ii) Sulphated iii) iv) Copper, Volatile percent ( final ) "C, Min ash, percent by mass, Max ppm, Max matter, by mass. 3400 ( Part 2 ) : 1980 (first Max Methods of test for natural .3660 ( Part 7 ) : 1988 rubber : Part 7 Determination of Imooney viscosity ( NR: 8 ) ( second revision ) Methods of test for natural .36~60 51 Determi( Part 51 ) : 1972 rubber : Part nation of ash, total copper, rubber hydromanganese, carbon, viscosity ( shearing viscometer ), and disk mixing and vulcanizing of in standard comrubber pound (first revision ) .4588 : 1!%6 6918 : 1972 v) Free amine, percent by mass, Max 0.75 Annex B Annex C vi) ;As;y,g;ent a) For uncoated material by 97.0 95.0 0.5 b) For coated/ bound material vii) Methanol insolubles, percent by mass, Annex D Max NOTES 1 The surface coated or bound material is likely contain approximately 2.0 percent of coating or binding material. The manufacturer should specify the solvent to be used for extracting in the binder. 2 In case of coated/uncoated material, the material shall be made free from binder by extracting with suitable solvent prior to testing for requirement ( vii ). Rubber, raw, natural ( rhird revision ) Mercaptobenzothiazole 1 3.2.1 All tests shall be carried out within 15 days of the receipt of the material by the purchaser. 3.3 Compoaodiag The material when compounded and tested according to the procedure given in Annex E shall have performance characteristics comparable to standard material satisfying the requirements of 3.1 and 3.2. 4 PACKING 4.1 Packing The material shall be packed securely so as to avoid exposure to air, moisture and acidic atmosphere. The exact mode of packing shall be as agreed to between the purchaser and the supplier. 4.2 Marking 4.2.1 Each package shall be marked -following: with the AND MARKING $2 Number of Tests 5.2.1 Test for copper ( see Table 1 ) shall beconducted on individual sample. 5.2.2 Test for all other characteristics conducted on a composite sample. 5.3 Criteria 5.3.1 Copper The mean and range of test results shall be calculated as follows: Mean ( X) = for copper for Conformity shall be. Thesum of test results Number of test results Range ( R ) = The difference between themaximum and minimum value of the test results The lot shall be deemed to have satisfied therequirement of the specification if: X + 0'6 20 5.3.2 Composite Samples In respect of all other characteristics the lot shall be considered as conforming to the specification if the composite samples satisfies each. of these requirements. 6 TEST METHODS a) Name of the material; b) Indication of source of manufacture; c) Net mass of the material; d) Month and year of the manufacture; e) Lot/batch number. 4.2.2 The packages Standard Mark. may also be marked and with 4.2.3 The use of Standard Mark is governed by the provisions of Bureau of Indian Standards Act, 1986 and the Rules and Regulations made thereunder. The details of conditions under which the licence for the use of Standard Mark may be granted to manufacturers or producers may be obtained from the Bureau of Indian Standards. 5 SAMPLING 5.1 The representative samples of the material shall be drawn as prescribed in IS 7086 ( Part 1 ) : 1973. 6.1 The tests shall be conducted according to the methods prescribed in Annex A to D and the relevant Indian Standard specification. Reference to relevant Annexes and Indian, Standard specification are given in co1 4 of Table 1. 6.2 Quality Reagent8 Unless specified otherwise, `pure chemicals' and, distilled water ( see IS 1070 : 1992 ) shall be employed in tests. NOTE - `Pure chemicals' shall mean that do not contain impurities which results of analysis. chemicals. affect the. ANNEX A [Tablel,Item (iv)] DETERMINATION A-l APPARATUS Glass Petri Dish 12 cm in OF VOLATILE MATTER A-3 CALCULATION Volatile matter, percent M1_ ~ C by mass 2 X 100` Ml diameter having 40 ml capacity. A-2 PROCEDURE Weigh 25 g, accurate to 1 mg, of the powdered material and spread it evenly on the dish. The dish is placed in an oven maintained at 65°C for one hour. The loss in mass is recorded. 2 where Ml = mass of the sample taken; and M2 = mass of the sample after heating. ANNEX B DETERMINATION B-l PROCEDURE 5 g of t$e material Weigh approximately accurately to 1 mg, and put in a 300-ml Erlenmeyer flask. Add 150 ml of isopropanol toiuene mixture ( 5 : 3 ) to dissolve the material. The solvent mixture of iSOprOpanol-tOlUene should be neutralized with respect to bromophenol blue to a greenish yellow end point before use. After adding a few drops of bromaphenol blue indicator the solution is titrated with 0'1 N hydrochloric acid till th6 appearance OF FREE AMINE of yellow colouration. B-2 CALCULATION Free amine, percent by mass = where V = volume 0'87 V M in ml of 0' 1 N chloric; acid used; and hydro- M = mass in g of the material takea for the test. ANNEX C [ Table 1, Item ( vi ) ] DETERMINATION C-l PROCEDURE Proceed as in B-l. Pass hydrogen sulphide gas for 15 to 20 minutes from the solution in which the free amine has been neutralized with 0'1 N hydrochloric acid. Titrate the liberated amine with 0'5 N hydrochloric acid till yellow colouration persists for one minute. C-2 CALCULATION Assay, percent by mass = 12.62 V M OF ASSAY where V = volume in ml of 0'5 N hydrochloric acid used; and M = mass in NOTE -If g of the material taken for the test. agreed to between the purchaser and spectrophotometric the supplier ultra-violet method may also be used. ANNEX D [ Table 1, Item (vii ) DETERMINATION D-l PROCEDURE D-l.1 Weigh 4 g of the material to the nearest milligram and put in a 400-ml beaker. Add 250 ml of methanol into it. Stir it at a room temperature for 30 minutes with the help of a magnetic stirrer. Allow the residue to settle. Decant the bulk of the supernatent liquid. Transfer the residue as thick slurry on to a previously weighed centered glass crucible (porosity No. 3 ). Wash the cake two or three times with 25 ml OF METHANOL 1 INSOLUBLES Dry tlie of methanol and then suck it dry. crucible at 100°C and weigh. D-1.2 I n case of granular/pellet material, material shall be powdered before testing. D-2 CALCULATION the Methanol insolubles, percent by mass = mass of the residue X Z 3 ks.l3%?1 : 1994 'ANNEX E .` ('Clause 3.3 ) METHODS E-1 TEST FOR COMPOUNDING AND TESTING MORPHOLINYL SULPHENAMIDE 3 TESTS OF BENZOTHIAZYL-N( MBS ) .T COMPOUND As a guidance, the following test compound may be used for -testing performance properties of benzothiazyl-N-morpholinyl sulphenamide ( MBS ) in rubber compound: Parts by Mass E-3.1 The tests given below are-recommended for each test sample. The approved sample shall also be tested side by side using the same master batch, that is, compound excluding accelerator only. E-3.1.1 Mooney scorch test shall be done at 120°C in accordance with the method prescribed in NR 8 of IS 3660 ( Part 7 ) : 1988. E-3.1.2 Tensile strength, modulus at 300 percent elongation, elongation at break at different cures at 141°C (from below to above the expected optimum cure ) shall be tested in accordance with the method described in IS 3400 (Part 1 ) : 1987. E-3.1.3 Hardness on optimum cure at 141°C shall be tested in accordance with the method prescribed in IS 3400 ( Part 2 ) : 1980. E-4 RESULT The values obtained with the test sample shall not vary by more than f20 percent for Mooney scorch and &-IO percent for all the other characteristics from those obtained with the approved sample. Natural rubber, Grade A ( conforming to IS 4588 : 1986 ) Carbon black, HAF Zinc oxide ( conforming to IS 3399 : 1993 ) Mineral oil ( aromatic ) plasticizer Stearic acid ( conforming IS 1675 : 1971 ) Sulphur ( conforming IS 8851 : 1994 ) to to 100 45 5 5 3 2'5, 0'5 Benzothiazyl-N-morpholinyl sulphenamide ( MBS ) E-2 COMPOUNDING Follow the procedure prescribed of IS 3660 ( Part 51 ) : 1972. in NR : 9 Bureau of Indian Standards BIS is a statutory institution established under the Bureau of Indian Standards -4ct, 1986 to promote harmonious development of the activities of standardization, marking and quality certification of goods and attending to connected matters in the country. Copyright BIS has a copyright of all its publications. No part of these publications may be reproduced in any form without the prior permission in writing of BIS. This does not preclude the free use, in the course of implementing the standard, of necessary details, such as symbols and sizes, type or grade designations. Enquiries relating to copyright be addressed to the Director ( Publications ), BIS. Review of Indian Standards Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed periodically; a standard along with amendments is reaffirmed when such a review indicates that no changes are needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of `BIS Handbook' and `Standards Monthly Addition'. This Indian Standard has been developed from Dot : No. PCD 13 ( 1120 ) Amendments Issued Since Publication Amend No. _ Date of Issue __.-___. 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